Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Narcis Avarvari' _publ_contact_author_address ; Department of Chemistry CNRS-Universite d'Angers 2 Bd. Lavoisier, UFR Sciences, B\^at. ANGERS 49045 FRANCE ; _publ_contact_author_email NARCIS.AVARVARI@UNIV-ANGERS.FR _publ_section_title ; Copper(I/II) complexes of a bis(tetrathiafulvalene) -2,2'-bipyridine : synthesis, characterization, magnetic and electrochemical properties ; loop_ _publ_author_name 'Narcis Avarvari' 'Patrick Batail' 'Rodolphe Clerac' 'Thomas Devic' 'Eric Levillain' 'David Rondeau' ; Y.Sahin ; data_L*2DMF-monoclinic _database_code_depnum_ccdc_archive 'CCDC 283136' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '2,2-bis(DMT-TTF-CONH-5-Py), 2DMF' _chemical_melting_point ? _chemical_formula_moiety C34H36N6O4S12 _chemical_formula_sum 'C34 H36 N6 O4 S12' _chemical_formula_weight 977.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.792(4) _cell_length_b 10.210(6) _cell_length_c 16.418(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.45(3) _cell_angle_gamma 90.00 _cell_volume 2180.0(15) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.8 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area_detector _diffrn_measurement_method 'rotation, phi incr. 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16767 _diffrn_reflns_av_R_equivalents 0.2071 _diffrn_reflns_av_sigmaI/netI 0.1777 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.17 _reflns_number_total 4141 _reflns_number_gt 1908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0328P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4141 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.10677(9) 0.93673(11) 0.16409(8) 0.0328(3) Uani 1 1 d . . . S2 S 0.24113(9) 0.85568(11) 0.06412(8) 0.0305(3) Uani 1 1 d . . . S3 S -0.09032(10) 0.80331(12) 0.01013(8) 0.0358(3) Uani 1 1 d . . . S4 S 0.05110(10) 0.73209(12) -0.08415(9) 0.0389(3) Uani 1 1 d . . . S5 S -0.27021(10) 0.66496(13) -0.11454(9) 0.0425(4) Uani 1 1 d . . . S6 S -0.10708(11) 0.58722(13) -0.22440(9) 0.0457(4) Uani 1 1 d . . . C1 C 0.2343(3) 0.9976(4) 0.1962(3) 0.0266(11) Uani 1 1 d . . . C2 C 0.2926(3) 0.9600(4) 0.1513(3) 0.0249(10) Uani 1 1 d . . . H2 H 0.3603 0.9888 0.1661 0.030 Uiso 1 1 calc R . . C3 C 0.1170(3) 0.8576(4) 0.0719(3) 0.0255(10) Uani 1 1 d . . . C4 C 0.0366(3) 0.8042(4) 0.0087(3) 0.0287(11) Uani 1 1 d . . . C5 C -0.1403(4) 0.7063(4) -0.0847(3) 0.0326(12) Uani 1 1 d . . . C6 C -0.0763(4) 0.6751(4) -0.1270(3) 0.0324(12) Uani 1 1 d . . . C7 C -0.2665(5) 0.5310(5) -0.0425(4) 0.066(2) Uani 1 1 d . . . H7A H -0.2280 0.4599 -0.0549 0.098 Uiso 1 1 calc R . . H7B H -0.3353 0.5024 -0.0503 0.098 Uiso 1 1 calc R . . H7C H -0.2341 0.5592 0.0161 0.098 Uiso 1 1 calc R . . C8 C -0.0373(5) 0.4380(5) -0.1885(4) 0.0546(16) Uani 1 1 d . . . H8A H 0.0332 0.4581 -0.1566 0.082 Uiso 1 1 calc R . . H8B H -0.0406 0.3849 -0.2376 0.082 Uiso 1 1 calc R . . H8C H -0.0672 0.3913 -0.1519 0.082 Uiso 1 1 calc R . . C9 C 0.2600(4) 1.0840(4) 0.2740(3) 0.0289(11) Uani 1 1 d . . . O1 O 0.1976(3) 1.0999(3) 0.3103(2) 0.0480(10) Uani 1 1 d . . . N1 N 0.3537(3) 1.1420(3) 0.2983(2) 0.0289(9) Uani 1 1 d . . . H1 H 0.3957 1.1158 0.2730 0.035 Uiso 1 1 calc R . . C10 C 0.3893(3) 1.2412(4) 0.3613(3) 0.0237(10) Uani 1 1 d . . . C11 C 0.3313(3) 1.3045(4) 0.4029(3) 0.0259(10) Uani 1 1 d . . . H11 H 0.2637 1.2793 0.3938 0.031 Uiso 1 1 calc R . . C12 C 0.3750(3) 1.4059(4) 0.4584(3) 0.0265(11) Uani 1 1 d . . . H12 H 0.3368 1.4491 0.4873 0.032 Uiso 1 1 calc R . . C13 C 0.4756(3) 1.4441(4) 0.4715(3) 0.0198(9) Uani 1 1 d . . . N2 N 0.5338(3) 1.3800(3) 0.4335(2) 0.0263(9) Uani 1 1 d . . . C14 C 0.4909(3) 1.2808(4) 0.3801(3) 0.0284(11) Uani 1 1 d . . . H14 H 0.5315 1.2359 0.3540 0.034 Uiso 1 1 calc R . . O2 O 0.4755(3) 0.9211(4) -0.2387(3) 0.0619(12) Uani 1 1 d . . . C15 C 0.3991(5) 0.9023(5) -0.2185(4) 0.0452(14) Uani 1 1 d . . . H15 H 0.3466 0.9639 -0.2366 0.054 Uiso 1 1 calc R . . N3 N 0.3844(3) 0.8008(4) -0.1727(3) 0.0392(11) Uani 1 1 d . . . C17 C 0.2924(4) 0.7884(6) -0.1489(4) 0.0533(15) Uani 1 1 d . . . H17A H 0.2500 0.8645 -0.1680 0.080 Uiso 1 1 calc R . . H17B H 0.3115 0.7808 -0.0873 0.080 Uiso 1 1 calc R . . H17C H 0.2550 0.7117 -0.1757 0.080 Uiso 1 1 calc R . . C16 C 0.4623(5) 0.7018(5) -0.1414(4) 0.0617(19) Uani 1 1 d . . . H16A H 0.4312 0.6167 -0.1529 0.093 Uiso 1 1 calc R . . H16B H 0.4954 0.7123 -0.0802 0.093 Uiso 1 1 calc R . . H16C H 0.5124 0.7105 -0.1700 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0261(6) 0.0380(7) 0.0351(7) -0.0128(6) 0.0112(5) -0.0091(5) S2 0.0250(7) 0.0331(6) 0.0327(7) -0.0118(5) 0.0086(5) -0.0052(5) S3 0.0255(7) 0.0424(7) 0.0391(8) -0.0117(6) 0.0103(5) -0.0060(5) S4 0.0279(7) 0.0500(7) 0.0365(8) -0.0158(6) 0.0077(5) -0.0071(6) S5 0.0245(7) 0.0482(8) 0.0466(8) 0.0016(6) 0.0009(6) -0.0059(6) S6 0.0424(8) 0.0475(8) 0.0366(8) -0.0140(6) -0.0011(6) -0.0001(6) C1 0.023(2) 0.019(2) 0.033(3) 0.0001(19) 0.004(2) -0.0041(18) C2 0.020(2) 0.024(2) 0.028(3) -0.0027(18) 0.005(2) -0.0027(18) C3 0.022(2) 0.023(2) 0.031(3) -0.0026(19) 0.009(2) -0.0035(18) C4 0.020(2) 0.030(2) 0.037(3) -0.004(2) 0.009(2) -0.0017(19) C5 0.028(3) 0.029(2) 0.034(3) -0.004(2) 0.002(2) -0.002(2) C6 0.025(3) 0.033(2) 0.032(3) -0.005(2) 0.000(2) -0.001(2) C7 0.054(4) 0.053(3) 0.083(5) 0.011(3) 0.013(4) -0.018(3) C8 0.051(4) 0.049(3) 0.061(4) -0.014(3) 0.015(3) 0.005(3) C9 0.023(3) 0.028(2) 0.036(3) -0.006(2) 0.010(2) -0.002(2) O1 0.039(2) 0.057(2) 0.051(2) -0.0304(18) 0.0199(19) -0.0221(18) N1 0.026(2) 0.0297(19) 0.032(2) -0.0110(17) 0.0108(18) -0.0085(17) C10 0.026(2) 0.019(2) 0.023(2) -0.0033(17) 0.0044(19) -0.0032(18) C11 0.020(2) 0.026(2) 0.029(3) -0.0082(19) 0.0055(19) -0.0051(19) C12 0.027(3) 0.022(2) 0.030(3) -0.0040(18) 0.009(2) 0.0017(18) C13 0.023(2) 0.018(2) 0.018(2) 0.0015(17) 0.0054(18) -0.0016(17) N2 0.022(2) 0.0267(19) 0.027(2) -0.0071(16) 0.0037(17) -0.0057(16) C14 0.023(3) 0.030(2) 0.031(3) -0.008(2) 0.009(2) -0.0017(19) O2 0.048(3) 0.077(3) 0.073(3) -0.035(2) 0.036(2) -0.019(2) C15 0.045(4) 0.050(3) 0.042(3) -0.021(3) 0.016(3) -0.005(3) N3 0.028(2) 0.045(2) 0.042(3) -0.015(2) 0.009(2) 0.0013(19) C17 0.044(4) 0.063(3) 0.053(4) -0.011(3) 0.016(3) -0.006(3) C16 0.044(4) 0.056(3) 0.076(5) -0.021(3) 0.007(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C3 1.763(5) . ? S1 C1 1.772(5) . ? S2 C2 1.735(4) . ? S2 C3 1.759(5) . ? S3 C4 1.758(5) . ? S3 C5 1.779(5) . ? S4 C6 1.760(5) . ? S4 C4 1.763(5) . ? S5 C5 1.745(5) . ? S5 C7 1.798(6) . ? S6 C6 1.758(5) . ? S6 C8 1.793(5) . ? C1 C2 1.317(7) . ? C1 C9 1.495(6) . ? C3 C4 1.355(6) . ? C5 C6 1.330(7) . ? C9 O1 1.209(6) . ? C9 N1 1.356(6) . ? O1 C11 2.864(5) . ? O1 C8 3.270(7) 4_576 ? N1 C10 1.413(5) . ? C10 C11 1.374(7) . ? C10 C14 1.391(6) . ? C11 C12 1.379(6) . ? C12 C13 1.386(6) . ? C13 N2 1.340(6) . ? C13 C13 1.489(8) 3_686 ? N2 C14 1.341(5) . ? N2 C12 2.833(5) 3_686 ? N2 C2 3.249(6) 2_655 ? O2 C15 1.221(7) . ? O2 N1 2.908(6) 3_675 ? O2 C14 3.250(6) 3_675 ? O2 C2 3.271(6) 3_675 ? C15 N3 1.335(7) . ? N3 C16 1.440(6) . ? N3 C17 1.451(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 S1 C1 93.5(2) . . ? C2 S2 C3 94.3(2) . . ? C4 S3 C5 95.0(2) . . ? C6 S4 C4 95.6(2) . . ? C5 S5 C7 101.4(3) . . ? C6 S6 C8 101.2(2) . . ? C2 C1 C9 129.4(4) . . ? C2 C1 S1 117.5(3) . . ? C9 C1 S1 113.0(4) . . ? C1 C2 S2 118.8(4) . . ? C4 C3 S2 120.5(4) . . ? C4 C3 S1 124.3(4) . . ? S2 C3 S1 115.2(2) . . ? C3 C4 S3 123.7(4) . . ? C3 C4 S4 122.0(4) . . ? S3 C4 S4 114.2(2) . . ? C6 C5 S5 126.4(4) . . ? C6 C5 S3 117.3(4) . . ? S5 C5 S3 116.2(3) . . ? C5 C6 S6 126.6(4) . . ? C5 C6 S4 117.3(4) . . ? S6 C6 S4 116.0(3) . . ? O1 C9 N1 124.1(4) . . ? O1 C9 C1 119.7(4) . . ? N1 C9 C1 116.2(4) . . ? C9 O1 C11 85.5(3) . . ? C9 O1 C8 148.8(3) . 4_576 ? C11 O1 C8 123.17(18) . 4_576 ? C9 N1 C10 126.4(4) . . ? C11 C10 C14 117.6(4) . . ? C11 C10 N1 125.6(4) . . ? C14 C10 N1 116.7(4) . . ? C10 C11 C12 118.9(4) . . ? C10 C11 O1 76.8(3) . . ? C12 C11 O1 164.0(4) . . ? C11 C12 C13 120.5(4) . . ? N2 C13 C12 120.9(4) . . ? N2 C13 C13 116.9(5) . 3_686 ? C12 C13 C13 122.2(5) . 3_686 ? C13 N2 C14 118.1(4) . . ? C13 N2 C12 62.7(2) . 3_686 ? C14 N2 C12 178.1(3) . 3_686 ? C13 N2 C2 135.9(3) . 2_655 ? C14 N2 C2 97.9(3) . 2_655 ? C12 N2 C2 80.67(15) 3_686 2_655 ? N2 C14 C10 123.8(4) . . ? C15 O2 N1 157.8(4) . 3_675 ? C15 O2 C14 115.8(3) . 3_675 ? N1 O2 C14 45.19(12) 3_675 3_675 ? C15 O2 C2 138.2(4) . 3_675 ? N1 O2 C2 56.43(13) 3_675 3_675 ? C14 O2 C2 101.42(16) 3_675 3_675 ? O2 C15 N3 125.6(6) . . ? C15 N3 C16 120.7(5) . . ? C15 N3 C17 122.0(5) . . ? C16 N3 C17 117.2(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C1 C9 O1 3.8(6) . . . . ? C2 C1 C9 O1 -174.6(5) . . . . ? C1 C9 N1 C10 170.3(4) . . . . ? O1 C9 N1 C10 -8.7(8) . . . . ? C9 N1 C10 C11 -6.4(7) . . . . ? C9 N1 C10 C14 176.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 26.17 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.781 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.109 #===END data_L*2DMF-triclinic _database_code_depnum_ccdc_archive 'CCDC 283137' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '2,2-bis(DMT-TTF-CONH-5-Py), 2DMF' _chemical_melting_point ? _chemical_formula_moiety C34H36N6O4S12 _chemical_formula_sum 'C34 H36 N6 O4 S12' _chemical_formula_weight 977.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6139(13) _cell_length_b 10.3442(12) _cell_length_c 12.8159(8) _cell_angle_alpha 89.901(7) _cell_angle_beta 71.596(9) _cell_angle_gamma 81.283(10) _cell_volume 1069.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.99 _cell_measurement_theta_max 11.57 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 506 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method w--2q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _diffrn_reflns_number 3510 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 23.99 _reflns_number_total 3271 _reflns_number_gt 1946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 [Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+1.8221P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3271 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1227 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.16127(18) 0.26536(14) 0.82832(10) 0.0441(4) Uani 1 1 d . . . S2 S 0.3998(2) 0.44134(15) 0.71959(11) 0.0514(4) Uani 1 1 d . . . S3 S 0.1767(2) 0.15605(15) 0.58587(11) 0.0523(4) Uani 1 1 d . . . S4 S 0.41436(19) 0.33214(14) 0.48185(11) 0.0500(4) Uani 1 1 d . . . S5 S 0.1928(2) 0.03094(17) 0.37188(13) 0.0626(5) Uani 1 1 d . . . S6 S 0.4769(2) 0.22513(17) 0.25350(11) 0.0595(5) Uani 1 1 d . . . O1 O 0.0339(5) 0.2866(4) 1.0624(3) 0.0496(10) Uani 1 1 d . . . N1 N 0.1834(5) 0.4323(4) 1.0997(3) 0.0432(11) Uani 1 1 d . . . H1 H 0.2604 0.4771 1.0684 0.052 Uiso 1 1 calc R . . C1 C 0.2163(6) 0.3722(5) 0.9127(4) 0.0345(12) Uani 1 1 d . . . C2 C 0.3245(6) 0.4500(5) 0.8604(4) 0.0406(13) Uani 1 1 d . . . H2 H 0.3585 0.5084 0.9004 0.049 Uiso 1 1 calc R . . C3 C 0.2847(6) 0.3196(5) 0.7044(4) 0.0375(12) Uani 1 1 d . . . C4 C 0.2933(6) 0.2735(5) 0.6048(4) 0.0396(13) Uani 1 1 d . . . C5 C 0.2646(7) 0.1395(5) 0.4408(4) 0.0441(14) Uani 1 1 d . . . C6 C 0.3752(7) 0.2197(6) 0.3947(4) 0.0460(14) Uani 1 1 d . . . C7 C 0.2564(10) -0.1209(6) 0.4256(6) 0.085(2) Uani 1 1 d . . . H7A H 0.3746 -0.1354 0.4087 0.128 Uiso 1 1 calc R . . H7B H 0.2238 -0.1912 0.3929 0.128 Uiso 1 1 calc R . . H7C H 0.2047 -0.1173 0.5040 0.128 Uiso 1 1 calc R . . C8 C 0.6783(9) 0.1479(9) 0.2468(6) 0.104(3) Uani 1 1 d . . . H8A H 0.7080 0.1819 0.3063 0.156 Uiso 1 1 calc R . . H8B H 0.7564 0.1646 0.1780 0.156 Uiso 1 1 calc R . . H8C H 0.6797 0.0552 0.2526 0.156 Uiso 1 1 calc R . . C9 C 0.1354(7) 0.3604(5) 1.0322(4) 0.0398(13) Uani 1 1 d . . . C10 C 0.1230(6) 0.4436(5) 1.2156(4) 0.0396(13) Uani 1 1 d . . . C11 C 0.0058(7) 0.3755(6) 1.2810(4) 0.0483(14) Uani 1 1 d . . . H11 H -0.0396 0.3160 1.2499 0.058 Uiso 1 1 calc R . . C12 C -0.0429(7) 0.3976(5) 1.3941(4) 0.0454(14) Uani 1 1 d . . . H12 H -0.1222 0.3528 1.4396 0.054 Uiso 1 1 calc R . . C13 C 0.0256(6) 0.4853(5) 1.4393(4) 0.0345(12) Uani 1 1 d . . . N2 N 0.1376(6) 0.5534(5) 1.3771(3) 0.0472(12) Uani 1 1 d . . . C14 C 0.1838(7) 0.5310(5) 1.2681(4) 0.0466(14) Uani 1 1 d . . . H14 H 0.2626 0.5777 1.2243 0.056 Uiso 1 1 calc R . . O2 O 0.3851(6) -0.3520(4) 0.0256(3) 0.0624(12) Uani 1 1 d . . . C15 C 0.2848(8) -0.2528(7) 0.0347(5) 0.0567(17) Uani 1 1 d . . . H15 H 0.1926 -0.2590 0.0133 0.068 Uiso 1 1 calc R . . N3 N 0.2961(6) -0.1370(5) 0.0725(4) 0.0575(13) Uani 1 1 d . . . C16 C 0.4434(9) -0.1252(7) 0.1030(6) 0.085(2) Uani 1 1 d . . . H16A H 0.4457 -0.1793 0.1637 0.127 Uiso 1 1 calc R . . H16B H 0.4403 -0.0356 0.1241 0.127 Uiso 1 1 calc R . . H16C H 0.5409 -0.1531 0.0413 0.127 Uiso 1 1 calc R . . C17 C 0.1691(10) -0.0263(8) 0.0832(7) 0.095(3) Uani 1 1 d . . . H17A H 0.0804 -0.0527 0.0623 0.143 Uiso 1 1 calc R . . H17B H 0.2142 0.0404 0.0362 0.143 Uiso 1 1 calc R . . H17C H 0.1275 0.0075 0.1582 0.143 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0555(9) 0.0542(9) 0.0241(7) -0.0007(6) -0.0081(6) -0.0230(7) S2 0.0629(10) 0.0640(10) 0.0280(7) 0.0004(6) -0.0064(7) -0.0297(8) S3 0.0647(10) 0.0634(10) 0.0305(7) 0.0001(7) -0.0091(7) -0.0286(8) S4 0.0657(11) 0.0557(9) 0.0278(7) 0.0009(6) -0.0077(7) -0.0233(8) S5 0.0805(12) 0.0683(11) 0.0472(9) -0.0086(8) -0.0264(8) -0.0239(9) S6 0.0752(12) 0.0733(11) 0.0252(7) -0.0001(7) -0.0073(7) -0.0160(9) O1 0.056(3) 0.064(3) 0.0300(19) -0.0020(18) -0.0094(18) -0.023(2) N1 0.051(3) 0.059(3) 0.021(2) -0.001(2) -0.008(2) -0.020(2) C1 0.042(3) 0.035(3) 0.025(3) 0.005(2) -0.010(2) -0.004(2) C2 0.051(3) 0.048(3) 0.022(3) -0.008(2) -0.009(2) -0.009(3) C3 0.046(3) 0.035(3) 0.029(3) 0.003(2) -0.005(2) -0.011(2) C4 0.042(3) 0.053(3) 0.024(3) 0.000(2) -0.012(2) -0.004(3) C5 0.049(3) 0.049(3) 0.033(3) -0.010(2) -0.014(3) -0.001(3) C6 0.049(4) 0.057(4) 0.032(3) -0.008(3) -0.009(3) -0.017(3) C7 0.094(6) 0.061(5) 0.102(6) -0.006(4) -0.029(5) -0.019(4) C8 0.076(6) 0.151(8) 0.053(5) -0.006(5) 0.007(4) 0.016(5) C9 0.041(3) 0.049(3) 0.024(3) 0.000(2) -0.003(2) -0.006(3) C10 0.041(3) 0.045(3) 0.032(3) 0.003(2) -0.011(2) -0.008(3) C11 0.061(4) 0.058(4) 0.029(3) -0.001(3) -0.011(3) -0.025(3) C12 0.052(4) 0.059(4) 0.020(3) 0.000(2) 0.002(2) -0.026(3) C13 0.039(3) 0.028(3) 0.032(3) -0.003(2) -0.006(2) -0.002(2) N2 0.053(3) 0.064(3) 0.028(2) -0.002(2) -0.012(2) -0.022(3) C14 0.052(4) 0.062(4) 0.030(3) 0.008(3) -0.007(3) -0.035(3) O2 0.085(3) 0.054(3) 0.053(3) -0.002(2) -0.024(2) -0.018(3) C15 0.057(4) 0.081(5) 0.041(3) 0.012(3) -0.021(3) -0.028(4) N3 0.053(3) 0.057(3) 0.062(3) -0.006(3) -0.022(3) 0.004(3) C16 0.084(6) 0.075(5) 0.104(6) -0.019(4) -0.047(5) -0.005(4) C17 0.093(6) 0.087(6) 0.107(6) 0.000(5) -0.048(5) 0.020(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C3 1.755(5) . ? S1 C1 1.762(5) . ? S2 C2 1.711(5) . ? S2 C3 1.763(5) . ? S3 C4 1.751(5) . ? S3 C5 1.769(5) . ? S4 C6 1.754(5) . ? S4 C4 1.758(5) . ? S5 C5 1.727(5) . ? S5 C7 1.793(7) . ? S6 C6 1.749(5) . ? S6 C8 1.773(8) . ? O1 C9 1.219(6) . ? O1 C11 2.876(6) . ? O1 C15 3.414(7) 2_556 ? N1 C9 1.339(6) . ? N1 C10 1.409(6) . ? C1 C2 1.340(7) . ? C1 C9 1.482(6) . ? C3 C4 1.339(6) . ? C5 C6 1.353(7) . ? C10 C11 1.377(7) . ? C10 C14 1.383(7) . ? C11 C12 1.385(7) . ? C12 C13 1.373(7) . ? C13 N2 1.334(6) . ? C13 C13 1.496(9) 2_568 ? N2 C14 1.337(6) . ? N2 C12 2.809(6) 2_568 ? O2 C15 1.217(7) . ? O2 N1 3.004(6) 1_544 ? O2 C2 3.161(6) 1_544 ? O2 C14 3.369(6) 1_544 ? C15 N3 1.322(8) . ? N3 C17 1.433(8) . ? N3 C16 1.462(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 S1 C1 94.7(2) . . ? C2 S2 C3 94.5(2) . . ? C4 S3 C5 96.0(2) . . ? C6 S4 C4 95.4(2) . . ? C5 S5 C7 100.9(3) . . ? C6 S6 C8 99.8(3) . . ? C9 O1 C11 85.0(3) . . ? C9 O1 C15 128.0(3) . 2_556 ? C11 O1 C15 126.6(2) . 2_556 ? C9 N1 C10 127.9(4) . . ? C2 C1 C9 130.0(5) . . ? C2 C1 S1 116.1(4) . . ? C9 C1 S1 113.9(4) . . ? C1 C2 S2 119.8(4) . . ? C4 C3 S1 123.6(4) . . ? C4 C3 S2 121.4(4) . . ? S1 C3 S2 114.9(3) . . ? C3 C4 S3 123.0(4) . . ? C3 C4 S4 122.7(4) . . ? S3 C4 S4 114.2(3) . . ? C6 C5 S5 126.5(4) . . ? C6 C5 S3 115.9(4) . . ? S5 C5 S3 117.5(3) . . ? C5 C6 S6 125.1(4) . . ? C5 C6 S4 117.9(4) . . ? S6 C6 S4 117.0(3) . . ? O1 C9 N1 124.7(4) . . ? O1 C9 C1 119.2(4) . . ? N1 C9 C1 116.0(5) . . ? C11 C10 C14 117.2(5) . . ? C11 C10 N1 125.0(5) . . ? C14 C10 N1 117.8(4) . . ? C10 C11 C12 118.6(5) . . ? C10 C11 O1 77.3(3) . . ? C12 C11 O1 164.0(4) . . ? C13 C12 C11 120.2(5) . . ? N2 C13 C12 122.0(4) . . ? N2 C13 C13 115.7(5) . 2_568 ? C12 C13 C13 122.2(6) . 2_568 ? C13 N2 C14 117.2(4) . . ? C13 N2 C12 63.4(3) . 2_568 ? C14 N2 C12 179.4(4) . 2_568 ? N2 C14 C10 124.7(5) . . ? C15 O2 N1 105.5(4) . 1_544 ? C15 O2 C2 107.5(4) . 1_544 ? N1 O2 C2 56.83(13) 1_544 1_544 ? C15 O2 C14 95.6(4) . 1_544 ? N1 O2 C14 43.59(12) 1_544 1_544 ? C2 O2 C14 100.38(17) 1_544 1_544 ? O2 C15 N3 125.4(6) . . ? C15 N3 C17 121.4(6) . . ? C15 N3 C16 117.7(5) . . ? C17 N3 C16 120.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C1 C9 O1 -4.0(7) . . . . ? C2 C1 C9 O1 176.7(5) . . . . ? C1 C9 N1 C10 177.4(5) . . . . ? O1 C9 N1 C10 -3.7(9) . . . . ? C9 N1 C10 C11 3.2(9) . . . . ? C9 N1 C10 C14 -175.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.348 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.080 #===END data_Cu(L) _database_code_depnum_ccdc_archive 'CCDC 283138' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (2,2-bis(DMT-TTF-CONH-3-Py))Cu(DMF)3(CF3SO3),2DMF _chemical_melting_point ? _chemical_formula_moiety C45H57CuF6N9O13S14 _chemical_formula_sum 'C45 H57 Cu F6 N9 O13 S14' _chemical_formula_weight 1558.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.764(2) _cell_length_b 28.797(3) _cell_length_c 14.6062(12) _cell_angle_alpha 90.00 _cell_angle_beta 122.316(7) _cell_angle_gamma 90.00 _cell_volume 7025.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 24.35 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3204 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area_detector _diffrn_measurement_method 'rotation, phi incr. 0.8' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58750 _diffrn_reflns_av_R_equivalents 0.1183 _diffrn_reflns_av_sigmaI/netI 0.2631 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.96 _reflns_number_total 13333 _reflns_number_gt 4306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(3.50(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.1261P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13333 _refine_ls_number_parameters 665 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1996 _refine_ls_R_factor_gt 0.0879 _refine_ls_wR_factor_ref 0.2667 _refine_ls_wR_factor_gt 0.2157 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.65998(6) 0.07870(4) 0.00067(10) 0.0473(3) Uani 1 1 d . . . S1 S 0.12791(12) -0.01466(8) -0.3179(2) 0.0488(6) Uani 1 1 d . . . S2 S 0.10140(14) 0.08650(9) -0.3132(3) 0.0639(8) Uani 1 1 d . . . S3 S -0.05895(13) -0.03297(10) -0.4049(2) 0.0597(7) Uani 1 1 d . . . S4 S -0.08476(15) 0.06766(11) -0.3976(3) 0.0676(8) Uani 1 1 d . . . S5 S -0.23352(15) -0.05492(14) -0.4950(3) 0.0879(11) Uani 1 1 d . . . S6 S -0.25826(19) 0.05531(17) -0.4715(4) 0.1119(16) Uani 1 1 d . . . C1 C 0.2110(4) 0.0225(3) -0.2654(7) 0.041(2) Uani 1 1 d . . . C2 C 0.1981(5) 0.0676(3) -0.2650(8) 0.055(3) Uani 1 1 d . . . H2 H 0.2400 0.0887 -0.2394 0.066 Uiso 1 1 calc R . . C3 C 0.0593(5) 0.0303(3) -0.3437(8) 0.049(2) Uani 1 1 d . . . C4 C -0.0177(5) 0.0229(4) -0.3773(8) 0.054(3) Uani 1 1 d . . . C5 C -0.1565(5) -0.0144(5) -0.4474(9) 0.062(3) Uani 1 1 d . . . C6 C -0.1673(6) 0.0316(5) -0.4431(10) 0.071(4) Uani 1 1 d . . . C7 C -0.1845(7) -0.1085(5) -0.4701(12) 0.093(4) Uani 1 1 d . . . H7A H -0.2230 -0.1332 -0.4942 0.139 Uiso 1 1 calc R . . H7B H -0.1460 -0.1118 -0.3939 0.139 Uiso 1 1 calc R . . H7C H -0.1576 -0.1099 -0.5087 0.139 Uiso 1 1 calc R . . C8 C -0.2831(7) 0.0928(5) -0.5792(11) 0.086(4) Uani 1 1 d . . . H8A H -0.3325 0.1083 -0.6011 0.130 Uiso 1 1 calc R . . H8B H -0.2890 0.0753 -0.6390 0.130 Uiso 1 1 calc R . . H8C H -0.2414 0.1154 -0.5566 0.130 Uiso 1 1 calc R . . C9 C 0.2879(5) -0.0014(3) -0.2213(7) 0.042(2) Uani 1 1 d . . . O1 O 0.2935(3) -0.0435(2) -0.2057(6) 0.0507(17) Uani 1 1 d . . . N1 N 0.3524(4) 0.0256(2) -0.1984(6) 0.046(2) Uani 1 1 d . . . H1 H 0.3435 0.0547 -0.2130 0.055 Uiso 1 1 calc R . . C10 C 0.4311(4) 0.0104(3) -0.1536(8) 0.042(2) Uani 1 1 d . . . C11 C 0.4539(5) -0.0357(3) -0.1530(8) 0.047(2) Uani 1 1 d . . . H11 H 0.4158 -0.0592 -0.1815 0.056 Uiso 1 1 calc R . . C12 C 0.5339(5) -0.0454(3) -0.1091(8) 0.049(3) Uani 1 1 d . . . H12 H 0.5500 -0.0761 -0.1055 0.059 Uiso 1 1 calc R . . C13 C 0.5897(4) -0.0109(3) -0.0709(7) 0.041(2) Uani 1 1 d . . . N2 N 0.5683(4) 0.0336(2) -0.0701(6) 0.0410(18) Uani 1 1 d . . . C14 C 0.4903(4) 0.0435(3) -0.1102(8) 0.043(2) Uani 1 1 d . . . H14 H 0.4762 0.0741 -0.1082 0.052 Uiso 1 1 calc R . . S7 S 1.11475(12) 0.05187(8) 0.1803(2) 0.0489(6) Uani 1 1 d . . . S8 S 1.18294(13) -0.04049(9) 0.1881(2) 0.0533(7) Uani 1 1 d . . . S9 S 1.29341(14) 0.09711(9) 0.2834(3) 0.0599(7) Uani 1 1 d . . . S10 S 1.35743(13) 0.00345(9) 0.2925(2) 0.0584(7) Uani 1 1 d . . . S11 S 1.45505(17) 0.14242(11) 0.3879(3) 0.0749(9) Uani 1 1 d . . . S12 S 1.52850(14) 0.03903(11) 0.4027(3) 0.0692(9) Uani 1 1 d . . . C15 C 1.0521(4) 0.0034(3) 0.1443(7) 0.039(2) Uani 1 1 d . . . C16 C 1.0838(5) -0.0381(3) 0.1477(8) 0.046(2) Uani 1 1 d . . . H16 H 1.0530 -0.0650 0.1288 0.055 Uiso 1 1 calc R . . C17 C 1.2005(5) 0.0191(3) 0.2161(8) 0.048(2) Uani 1 1 d . . . C18 C 1.2733(5) 0.0378(3) 0.2593(8) 0.050(2) Uani 1 1 d . . . C19 C 1.3972(5) 0.0920(4) 0.3418(9) 0.053(3) Uani 1 1 d . . . C20 C 1.4266(5) 0.0493(3) 0.3455(8) 0.049(2) Uani 1 1 d . . . C21 C 1.4695(10) 0.1546(5) 0.2797(15) 0.120(6) Uani 1 1 d . . . H21A H 1.5009 0.1824 0.2959 0.180 Uiso 1 1 calc R . . H21B H 1.4185 0.1589 0.2138 0.180 Uiso 1 1 calc R . . H21C H 1.4970 0.1291 0.2712 0.180 Uiso 1 1 calc R . . C22 C 1.5327(6) -0.0225(4) 0.3844(10) 0.071(3) Uani 1 1 d . . . H22A H 1.5873 -0.0316 0.4139 0.107 Uiso 1 1 calc R . . H22B H 1.5014 -0.0297 0.3086 0.107 Uiso 1 1 calc R . . H22C H 1.5117 -0.0389 0.4211 0.107 Uiso 1 1 calc R . . O2 O 0.9489(3) 0.0553(2) 0.1050(6) 0.0518(17) Uani 1 1 d . . . N3 N 0.9177(4) -0.0220(2) 0.0821(6) 0.0442(19) Uani 1 1 d . . . H3 H 0.9375 -0.0493 0.0893 0.053 Uiso 1 1 calc R . . C23 C 0.9685(5) 0.0145(3) 0.1089(7) 0.043(2) Uani 1 1 d . . . C24 C 0.8356(4) -0.0192(3) 0.0438(7) 0.041(2) Uani 1 1 d . . . C25 C 0.7913(5) -0.0599(3) 0.0094(8) 0.044(2) Uani 1 1 d . . . H25 H 0.8156 -0.0879 0.0110 0.052 Uiso 1 1 calc R . . C26 C 0.7111(5) -0.0586(3) -0.0271(8) 0.044(2) Uani 1 1 d . . . H26 H 0.6809 -0.0857 -0.0501 0.053 Uiso 1 1 calc R . . C27 C 0.6759(4) -0.0172(3) -0.0295(7) 0.036(2) Uani 1 1 d . . . N4 N 0.7199(4) 0.0220(2) 0.0044(6) 0.0411(18) Uani 1 1 d . . . C28 C 0.7985(4) 0.0216(3) 0.0415(8) 0.042(2) Uani 1 1 d . . . H28 H 0.8280 0.0489 0.0658 0.050 Uiso 1 1 calc R . . O3 O 0.7595(3) 0.1152(2) 0.0899(6) 0.0488(16) Uani 1 1 d . . . C29 C 0.7856(5) 0.1274(3) 0.1849(9) 0.051(3) Uani 1 1 d . . . H29 H 0.7512 0.1258 0.2101 0.061 Uiso 1 1 calc R . . N5 N 0.8584(5) 0.1425(3) 0.2514(7) 0.057(2) Uani 1 1 d . . . C30 C 0.9158(6) 0.1452(4) 0.2190(10) 0.078(4) Uani 1 1 d . . . H30A H 0.9657 0.1570 0.2781 0.118 Uiso 1 1 calc R . . H30B H 0.8959 0.1656 0.1579 0.118 Uiso 1 1 calc R . . H30C H 0.9240 0.1148 0.1996 0.118 Uiso 1 1 calc R . . C31 C 0.8875(9) 0.1545(6) 0.3644(12) 0.117(6) Uani 1 1 d . . . H31A H 0.9421 0.1648 0.4000 0.176 Uiso 1 1 calc R . . H31B H 0.8846 0.1276 0.4010 0.176 Uiso 1 1 calc R . . H31C H 0.8550 0.1788 0.3660 0.176 Uiso 1 1 calc R . . O4 O 0.5963(3) 0.12360(19) 0.0228(6) 0.0567(19) Uani 1 1 d . . . C32 C 0.5990(6) 0.1667(4) 0.0150(9) 0.061(3) Uani 1 1 d . . . H32 H 0.6244 0.1786 -0.0181 0.073 Uiso 1 1 calc R . . N6 N 0.5686(6) 0.1953(3) 0.0503(9) 0.069(3) Uani 1 1 d . . . C33 C 0.5730(11) 0.2460(4) 0.0451(16) 0.121(6) Uani 1 1 d . . . H33A H 0.5466 0.2602 0.0773 0.182 Uiso 1 1 calc R . . H33B H 0.5472 0.2556 -0.0292 0.182 Uiso 1 1 calc R . . H33C H 0.6281 0.2555 0.0838 0.182 Uiso 1 1 calc R . . C34 C 0.5296(10) 0.1782(4) 0.1053(15) 0.109(6) Uani 1 1 d . . . H34A H 0.5106 0.2040 0.1269 0.164 Uiso 1 1 calc R . . H34B H 0.5674 0.1607 0.1682 0.164 Uiso 1 1 calc R . . H34C H 0.4853 0.1586 0.0569 0.164 Uiso 1 1 calc R . . O5 O 0.6427(4) 0.1083(2) -0.1495(6) 0.0634(19) Uani 1 1 d . . . C35 C 0.6976(6) 0.1269(3) -0.1546(11) 0.064(3) Uani 1 1 d . . . H35 H 0.7441 0.1340 -0.0889 0.077 Uiso 1 1 calc R . . N7 N 0.6971(5) 0.1372(3) -0.2403(9) 0.066(2) Uani 1 1 d . . . C36 C 0.7645(8) 0.1594(5) -0.2341(13) 0.097(4) Uani 1 1 d . . . H36A H 0.7531 0.1646 -0.3060 0.145 Uiso 1 1 calc R . . H36B H 0.8108 0.1399 -0.1950 0.145 Uiso 1 1 calc R . . H36C H 0.7746 0.1886 -0.1973 0.145 Uiso 1 1 calc R . . C37 C 0.6287(8) 0.1287(4) -0.3467(11) 0.092(4) Uani 1 1 d . . . H37A H 0.6398 0.1388 -0.3999 0.138 Uiso 1 1 calc R . . H37B H 0.5834 0.1455 -0.3559 0.138 Uiso 1 1 calc R . . H37C H 0.6169 0.0960 -0.3555 0.138 Uiso 1 1 calc R . . S13 S 0.3067(3) 0.72994(15) 0.1120(5) 0.1333(18) Uani 1 1 d D . . O6 O 0.3424(7) 0.7717(4) 0.1439(11) 0.141(4) Uiso 1 1 d D . . O7 O 0.3444(8) 0.6976(5) 0.0717(12) 0.155(5) Uiso 1 1 d . . . O8 O 0.2852(8) 0.7061(5) 0.1810(11) 0.148(4) Uiso 1 1 d . . . C38 C 0.2220(15) 0.7388(9) 0.006(2) 0.161(8) Uiso 1 1 d . . . F1 F 0.1738(8) 0.6989(5) -0.0499(11) 0.173(4) Uiso 1 1 d . . . F2 F 0.1726(9) 0.7681(6) 0.0123(13) 0.205(6) Uiso 1 1 d . . . F3 F 0.2240(8) 0.7564(5) -0.0841(12) 0.183(5) Uiso 1 1 d . . . S14 S 0.2846(4) 0.3162(2) -0.5724(6) 0.151(2) Uani 1 1 d D . . O11 O 0.3469(12) 0.3466(7) -0.5583(18) 0.230(8) Uiso 1 1 d D . . O12 O 0.2177(9) 0.3277(5) -0.6675(13) 0.154(5) Uiso 1 1 d . . . O13 O 0.2608(18) 0.3192(11) -0.502(2) 0.324(14) Uiso 1 1 d D . . C45 C 0.309(2) 0.2606(12) -0.588(3) 0.208(12) Uiso 1 1 d . . . F4 F 0.375(3) 0.2559(17) -0.520(5) 0.53(3) Uiso 1 1 d . . . F5 F 0.244(2) 0.2316(12) -0.605(3) 0.384(15) Uiso 1 1 d . . . F6 F 0.3248(18) 0.2581(10) -0.674(3) 0.369(14) Uiso 1 1 d . . . O9 O 0.9603(5) 0.8807(3) 0.0892(7) 0.075(2) Uiso 1 1 d . . . C39 C 0.9521(11) 0.8516(6) 0.1473(15) 0.122(6) Uiso 1 1 d . . . H39 H 0.9065 0.8569 0.1495 0.146 Uiso 1 1 calc R . . N8 N 0.9934(11) 0.8156(7) 0.2052(16) 0.160(6) Uiso 1 1 d . . . C40 C 1.0644(13) 0.8030(8) 0.1980(18) 0.272(16) Uiso 1 1 d . . . H40A H 1.0911 0.7766 0.2432 0.409 Uiso 1 1 calc R . . H40B H 1.1008 0.8288 0.2218 0.409 Uiso 1 1 calc R . . H40C H 1.0465 0.7956 0.1243 0.409 Uiso 1 1 calc R . . C41 C 0.9664(13) 0.7781(8) 0.2575(18) 0.225(12) Uiso 1 1 d R . . H41A H 1.0079 0.7552 0.2941 0.337 Uiso 1 1 calc R . . H41B H 0.9182 0.7634 0.2018 0.337 Uiso 1 1 calc R . . H41C H 0.9568 0.7928 0.3084 0.337 Uiso 1 1 calc R . . O10 O 0.3574(8) 0.1122(5) -0.2745(11) 0.150(4) Uiso 1 1 d . . . C42 C 0.3790(8) 0.1531(5) -0.2559(11) 0.166(8) Uiso 1 1 d . . . H42 H 0.3672 0.1699 -0.2117 0.011(15) Uiso 1 1 calc R . . N9 N 0.4171(8) 0.1747(5) -0.2937(11) 0.159(6) Uiso 1 1 d R . . C43 C 0.4435(8) 0.2219(5) -0.2622(11) 0.298(19) Uiso 1 1 d R . . H43A H 0.4705 0.2323 -0.2970 0.447 Uiso 1 1 calc R . . H43B H 0.4796 0.2235 -0.1851 0.447 Uiso 1 1 calc R . . H43C H 0.3980 0.2415 -0.2836 0.447 Uiso 1 1 calc R . . C44 C 0.4284(19) 0.1552(11) -0.366(3) 0.241(14) Uiso 1 1 d . . . H44A H 0.4595 0.1755 -0.3819 0.362 Uiso 1 1 calc R . . H44B H 0.3775 0.1494 -0.4316 0.362 Uiso 1 1 calc R . . H44C H 0.4564 0.1263 -0.3384 0.362 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0246(5) 0.0335(5) 0.0747(9) -0.0131(6) 0.0205(5) -0.0034(4) S1 0.0254(10) 0.0505(13) 0.0602(17) -0.0033(12) 0.0160(11) -0.0029(9) S2 0.0385(12) 0.0558(16) 0.085(2) 0.0006(14) 0.0250(13) 0.0085(11) S3 0.0276(10) 0.0754(18) 0.0716(19) 0.0070(14) 0.0235(12) 0.0014(11) S4 0.0464(13) 0.082(2) 0.078(2) 0.0170(16) 0.0361(14) 0.0203(13) S5 0.0345(13) 0.125(3) 0.098(3) 0.023(2) 0.0315(15) -0.0066(15) S6 0.0588(18) 0.164(4) 0.142(4) 0.073(3) 0.073(2) 0.054(2) C1 0.025(4) 0.050(5) 0.045(6) -0.004(4) 0.016(4) -0.001(4) C2 0.034(4) 0.050(6) 0.065(7) -0.004(5) 0.017(5) -0.008(4) C3 0.029(4) 0.068(6) 0.041(6) -0.003(5) 0.013(4) 0.001(4) C4 0.034(4) 0.080(7) 0.048(6) 0.014(5) 0.021(4) 0.015(5) C5 0.025(4) 0.106(9) 0.061(7) 0.020(6) 0.026(5) 0.002(5) C6 0.040(5) 0.103(10) 0.085(9) 0.043(7) 0.042(6) 0.022(6) C7 0.058(7) 0.099(10) 0.117(12) -0.004(9) 0.044(8) -0.013(7) C8 0.054(6) 0.111(10) 0.087(10) 0.001(8) 0.033(6) 0.014(6) C9 0.035(4) 0.039(5) 0.049(6) -0.011(4) 0.021(4) -0.001(4) O1 0.038(3) 0.039(4) 0.073(5) -0.006(3) 0.029(3) -0.003(3) N1 0.023(3) 0.036(4) 0.065(5) 0.002(4) 0.014(3) -0.003(3) C10 0.020(4) 0.043(5) 0.053(6) -0.005(4) 0.011(4) -0.002(3) C11 0.028(4) 0.042(5) 0.060(7) -0.014(5) 0.017(4) -0.013(4) C12 0.033(4) 0.027(4) 0.078(7) -0.010(5) 0.023(5) -0.001(3) C13 0.027(4) 0.042(5) 0.053(6) -0.011(4) 0.021(4) -0.003(4) N2 0.027(3) 0.030(4) 0.059(5) -0.006(3) 0.018(3) -0.002(3) C14 0.021(4) 0.032(4) 0.062(6) -0.006(4) 0.013(4) 0.000(3) S7 0.0303(10) 0.0510(14) 0.0660(18) 0.0023(12) 0.0260(11) 0.0060(9) S8 0.0340(11) 0.0533(14) 0.081(2) 0.0110(13) 0.0366(12) 0.0105(10) S9 0.0412(12) 0.0559(15) 0.085(2) 0.0047(14) 0.0357(14) 0.0062(11) S10 0.0326(11) 0.0560(15) 0.091(2) 0.0099(14) 0.0357(13) 0.0073(10) S11 0.0607(16) 0.0692(18) 0.093(2) -0.0093(17) 0.0399(17) -0.0128(14) S12 0.0311(12) 0.084(2) 0.093(2) 0.0122(17) 0.0335(14) 0.0029(12) C15 0.023(4) 0.051(5) 0.046(6) -0.003(4) 0.020(4) 0.003(4) C16 0.031(4) 0.056(6) 0.059(7) 0.006(5) 0.029(4) 0.008(4) C17 0.036(4) 0.060(6) 0.055(6) 0.003(5) 0.029(4) 0.005(4) C18 0.030(4) 0.063(6) 0.063(7) 0.005(5) 0.029(5) 0.006(4) C19 0.039(5) 0.063(6) 0.067(7) 0.000(5) 0.035(5) -0.004(4) C20 0.033(4) 0.060(6) 0.059(7) 0.012(5) 0.027(4) 0.001(4) C21 0.138(13) 0.080(10) 0.166(17) -0.010(10) 0.098(13) -0.038(9) C22 0.039(5) 0.083(8) 0.099(10) 0.019(7) 0.042(6) 0.017(5) O2 0.029(3) 0.050(4) 0.070(5) -0.008(3) 0.022(3) 0.003(3) N3 0.028(3) 0.042(4) 0.064(5) 0.001(4) 0.026(4) 0.007(3) C23 0.029(4) 0.057(6) 0.044(6) -0.002(5) 0.020(4) 0.008(4) C24 0.028(4) 0.052(5) 0.038(6) -0.008(4) 0.015(4) 0.002(4) C25 0.034(4) 0.035(5) 0.060(6) -0.006(4) 0.024(4) 0.009(4) C26 0.036(4) 0.037(5) 0.055(6) -0.007(4) 0.022(4) -0.001(4) C27 0.029(4) 0.027(4) 0.052(6) -0.006(4) 0.021(4) 0.000(3) N4 0.030(3) 0.036(4) 0.055(5) -0.011(3) 0.021(3) -0.003(3) C28 0.024(4) 0.038(5) 0.058(6) -0.003(4) 0.019(4) 0.001(3) O3 0.040(3) 0.039(3) 0.064(5) -0.013(3) 0.025(3) -0.005(3) C29 0.040(5) 0.041(5) 0.072(8) -0.012(5) 0.031(5) -0.017(4) N5 0.055(5) 0.054(5) 0.063(6) -0.014(4) 0.032(5) -0.019(4) C30 0.043(5) 0.091(9) 0.091(9) -0.041(7) 0.029(6) -0.015(6) C31 0.122(12) 0.151(14) 0.095(12) -0.069(10) 0.070(10) -0.088(11) O4 0.040(3) 0.025(3) 0.106(6) -0.011(3) 0.039(4) -0.007(2) C32 0.044(5) 0.059(7) 0.080(8) 0.004(6) 0.032(6) 0.006(5) N6 0.087(6) 0.038(4) 0.106(8) -0.002(5) 0.067(6) 0.008(4) C33 0.194(17) 0.033(6) 0.211(19) 0.005(9) 0.159(16) 0.007(8) C34 0.174(15) 0.050(7) 0.192(17) -0.017(9) 0.157(15) -0.004(8) O5 0.044(4) 0.050(4) 0.078(5) 0.000(4) 0.020(4) -0.001(3) C35 0.052(6) 0.041(6) 0.071(9) -0.003(6) 0.014(6) -0.002(5) N7 0.064(6) 0.053(5) 0.075(8) 0.005(5) 0.034(6) -0.007(4) C36 0.100(10) 0.086(9) 0.104(12) 0.007(8) 0.055(9) -0.013(8) C37 0.092(9) 0.073(8) 0.087(11) 0.019(7) 0.031(8) -0.012(7) S13 0.142(4) 0.078(3) 0.191(6) -0.004(3) 0.096(4) -0.017(3) S14 0.125(4) 0.136(4) 0.163(5) -0.034(4) 0.059(4) 0.043(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4 1.949(6) . ? Cu1 O3 1.982(6) . ? Cu1 N4 1.999(7) . ? Cu1 N2 2.010(6) . ? Cu1 O5 2.203(8) . ? Cu1 O1 2.811(7) 3_655 ? S1 C1 1.757(8) . ? S1 C3 1.764(9) . ? S2 C2 1.733(9) . ? S2 C3 1.765(10) . ? S3 C4 1.750(11) . ? S3 C5 1.764(9) . ? S4 C6 1.739(12) . ? S4 C4 1.756(10) . ? S5 C5 1.740(11) . ? S5 C7 1.755(14) . ? S6 C8 1.747(14) . ? S6 C6 1.753(10) . ? C1 C2 1.324(12) . ? C1 C9 1.467(11) . ? C2 O10 3.470(16) . ? C3 C4 1.343(12) . ? C5 C6 1.349(16) . ? C9 O1 1.226(10) . ? C9 N1 1.373(10) . ? O1 C11 2.842(10) . ? O1 C29 2.982(10) 3_655 ? O1 C8 3.353(15) 3_554 ? N1 C10 1.397(9) . ? N1 O10 2.754(16) . ? C10 C14 1.374(11) . ? C10 C11 1.398(12) . ? C11 C12 1.382(11) . ? C12 C13 1.362(11) . ? C13 N2 1.353(10) . ? C13 C27 1.482(10) . ? N2 C14 1.354(9) . ? C14 O4 3.022(10) . ? C14 O10 3.136(16) . ? S7 C15 1.749(9) . ? S7 C17 1.758(8) . ? S8 C16 1.719(8) . ? S8 C17 1.756(10) . ? S9 C18 1.746(10) . ? S9 C19 1.757(9) . ? S10 C20 1.755(10) . ? S10 C18 1.765(9) . ? S11 C19 1.744(10) . ? S11 C21 1.785(16) . ? S12 C20 1.743(8) . ? S12 C22 1.799(12) . ? C15 C16 1.339(12) . ? C15 C23 1.479(10) . ? C17 C18 1.336(12) . ? C19 C20 1.350(13) . ? O2 C23 1.229(10) . ? O2 C28 2.772(9) . ? O2 C30 3.328(13) . ? N3 C23 1.358(11) . ? N3 C24 1.406(9) . ? C24 C28 1.374(11) . ? C24 C25 1.388(12) . ? C25 C26 1.376(11) . ? C26 C27 1.371(11) . ? C27 N4 1.348(10) . ? N4 C28 1.345(9) . ? O3 C29 1.245(11) . ? O3 C35 3.115(16) . ? C29 N5 1.307(11) . ? N5 C30 1.447(13) . ? N5 C31 1.469(15) . ? O4 C32 1.251(11) . ? C32 N6 1.278(13) . ? N6 C34 1.464(14) . ? N6 C33 1.469(14) . ? O5 C35 1.248(13) . ? C35 N7 1.280(14) . ? N7 C37 1.435(16) . ? N7 C36 1.436(15) . ? S13 O6 1.345(12) . ? S13 O8 1.458(14) . ? S13 O7 1.497(15) . ? S13 C38 1.58(3) . ? O6 C32 3.570(17) 3_665 ? O8 C31 3.45(2) 2_655 ? C38 F2 1.33(2) . ? C38 F3 1.43(2) . ? C38 F1 1.44(2) . ? S14 O13 1.341(17) . ? S14 O12 1.350(15) . ? S14 O11 1.434(15) . ? S14 C45 1.73(3) . ? O11 C34 3.17(3) 4_565 ? O11 C42 3.27(3) 4_565 ? C45 F4 1.15(5) . ? C45 F6 1.43(4) . ? C45 F5 1.45(4) . ? O9 C39 1.264(18) . ? O9 N3 2.911(11) 1_565 ? O9 C16 3.150(12) 1_565 ? O9 C25 3.357(11) 1_565 ? C39 N8 1.31(2) . ? N8 C40 1.51(3) . ? N8 C41 1.57(3) . ? O10 C42 1.235(18) . ? C42 N9 1.3044 . ? N9 C44 1.32(3) . ? N9 C43 1.4423 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cu1 O3 92.3(2) . . ? O4 Cu1 N4 164.3(3) . . ? O3 Cu1 N4 92.9(2) . . ? O4 Cu1 N2 91.7(2) . . ? O3 Cu1 N2 170.3(3) . . ? N4 Cu1 N2 81.0(3) . . ? O4 Cu1 O5 98.0(3) . . ? O3 Cu1 O5 91.2(3) . . ? N4 Cu1 O5 96.7(3) . . ? N2 Cu1 O5 96.9(3) . . ? O4 Cu1 O1 86.3(3) . 3_655 ? O3 Cu1 O1 81.1(2) . 3_655 ? N4 Cu1 O1 79.9(3) . 3_655 ? N2 Cu1 O1 90.3(3) . 3_655 ? O5 Cu1 O1 171.4(2) . 3_655 ? C1 S1 C3 94.5(4) . . ? C2 S2 C3 94.8(4) . . ? C4 S3 C5 95.1(5) . . ? C6 S4 C4 95.4(5) . . ? C5 S5 C7 103.8(5) . . ? C8 S6 C6 102.3(5) . . ? C2 C1 C9 128.1(8) . . ? C2 C1 S1 117.5(6) . . ? C9 C1 S1 114.3(6) . . ? C1 C2 S2 118.6(7) . . ? C1 C2 O10 100.4(6) . . ? S2 C2 O10 134.0(5) . . ? C4 C3 S1 123.6(8) . . ? C4 C3 S2 121.8(8) . . ? S1 C3 S2 114.5(4) . . ? C3 C4 S3 121.8(8) . . ? C3 C4 S4 123.4(8) . . ? S3 C4 S4 114.8(5) . . ? C6 C5 S5 123.4(7) . . ? C6 C5 S3 116.8(8) . . ? S5 C5 S3 119.7(8) . . ? C5 C6 S4 117.7(7) . . ? C5 C6 S6 122.7(8) . . ? S4 C6 S6 119.4(8) . . ? O1 C9 N1 122.3(7) . . ? O1 C9 C1 121.0(7) . . ? N1 C9 C1 116.7(8) . . ? C9 O1 C11 87.1(5) . . ? C9 O1 C29 145.0(5) . 3_655 ? C11 O1 C29 127.3(3) . 3_655 ? C9 O1 C8 106.8(6) . 3_554 ? C11 O1 C8 77.8(3) . 3_554 ? C29 O1 C8 88.8(4) 3_655 3_554 ? C9 N1 C10 126.4(7) . . ? C9 N1 O10 130.0(6) . . ? C10 N1 O10 101.6(6) . . ? C14 C10 N1 117.3(7) . . ? C14 C10 C11 117.6(7) . . ? N1 C10 C11 125.0(7) . . ? C12 C11 C10 118.7(7) . . ? C12 C11 O1 160.7(7) . . ? C10 C11 O1 76.4(5) . . ? C13 C12 C11 121.1(8) . . ? N2 C13 C12 120.4(7) . . ? N2 C13 C27 114.2(7) . . ? C12 C13 C27 125.5(7) . . ? C13 N2 C14 119.0(6) . . ? C13 N2 Cu1 114.6(5) . . ? C14 N2 Cu1 126.2(5) . . ? N2 C14 C10 123.0(7) . . ? N2 C14 O4 69.2(4) . . ? C10 C14 O4 162.4(7) . . ? N2 C14 O10 139.3(7) . . ? C10 C14 O10 85.8(6) . . ? O4 C14 O10 91.1(4) . . ? C15 S7 C17 94.4(4) . . ? C16 S8 C17 95.1(4) . . ? C18 S9 C19 95.6(4) . . ? C20 S10 C18 95.6(4) . . ? C19 S11 C21 101.8(6) . . ? C20 S12 C22 103.2(5) . . ? C16 C15 C23 128.2(8) . . ? C16 C15 S7 117.4(6) . . ? C23 C15 S7 114.4(6) . . ? C15 C16 S8 118.2(7) . . ? C18 C17 S8 122.2(7) . . ? C18 C17 S7 123.2(8) . . ? S8 C17 S7 114.6(5) . . ? C17 C18 S9 124.1(7) . . ? C17 C18 S10 121.5(8) . . ? S9 C18 S10 114.4(5) . . ? C20 C19 S11 124.3(7) . . ? C20 C19 S9 117.5(7) . . ? S11 C19 S9 118.2(6) . . ? C19 C20 S12 122.4(7) . . ? C19 C20 S10 116.8(6) . . ? S12 C20 S10 120.8(6) . . ? C23 O2 C28 86.3(5) . . ? C23 O2 C30 149.6(7) . . ? C28 O2 C30 88.7(3) . . ? C23 N3 C24 126.0(7) . . ? O2 C23 N3 124.1(7) . . ? O2 C23 C15 119.2(8) . . ? N3 C23 C15 116.8(8) . . ? C28 C24 C25 119.2(7) . . ? C28 C24 N3 123.0(8) . . ? C25 C24 N3 117.7(7) . . ? C26 C25 C24 119.3(7) . . ? C27 C26 C25 119.9(8) . . ? N4 C27 C26 120.1(7) . . ? N4 C27 C13 114.9(6) . . ? C26 C27 C13 125.0(7) . . ? C28 N4 C27 121.2(7) . . ? C28 N4 Cu1 124.0(5) . . ? C27 N4 Cu1 114.7(5) . . ? N4 C28 C24 120.3(7) . . ? N4 C28 O2 158.8(6) . . ? C24 C28 O2 80.1(5) . . ? C29 O3 Cu1 123.9(6) . . ? C29 O3 C35 157.2(6) . . ? Cu1 O3 C35 70.1(3) . . ? O3 C29 N5 123.9(9) . . ? C29 N5 C30 121.3(9) . . ? C29 N5 C31 121.8(9) . . ? C30 N5 C31 116.7(9) . . ? N5 C30 O2 121.3(7) . . ? C32 O4 Cu1 125.5(6) . . ? C32 O4 C14 138.4(7) . . ? Cu1 O4 C14 71.0(2) . . ? O4 C32 N6 123.3(10) . . ? C32 N6 C34 120.3(9) . . ? C32 N6 C33 124.4(10) . . ? C34 N6 C33 115.2(9) . . ? C35 O5 Cu1 123.3(7) . . ? O5 C35 N7 127.2(11) . . ? O5 C35 O3 72.9(7) . . ? N7 C35 O3 159.9(8) . . ? C35 N7 C37 121.9(10) . . ? C35 N7 C36 121.3(11) . . ? C37 N7 C36 116.7(11) . . ? O6 S13 O8 118.3(9) . . ? O6 S13 O7 114.4(9) . . ? O8 S13 O7 111.8(8) . . ? O6 S13 C38 106.3(11) . . ? O8 S13 C38 101.9(11) . . ? O7 S13 C38 101.9(12) . . ? S13 O6 C32 120.8(8) . 3_665 ? S13 O8 C31 134.0(8) . 2_655 ? F2 C38 F3 103(2) . . ? F2 C38 F1 105(2) . . ? F3 C38 F1 95.5(18) . . ? F2 C38 S13 118(2) . . ? F3 C38 S13 115.0(18) . . ? F1 C38 S13 117.5(18) . . ? O13 S14 O12 102.8(15) . . ? O13 S14 O11 118.4(17) . . ? O12 S14 O11 107.0(12) . . ? O13 S14 C45 114(2) . . ? O12 S14 C45 106.3(15) . . ? O11 S14 C45 107.5(16) . . ? S14 O11 C34 121.1(11) . 4_565 ? S14 O11 C42 115.6(12) . 4_565 ? C34 O11 C42 89.2(6) 4_565 4_565 ? F4 C45 F6 94(4) . . ? F4 C45 F5 125(5) . . ? F6 C45 F5 114(3) . . ? F4 C45 S14 105(4) . . ? F6 C45 S14 112(3) . . ? F5 C45 S14 105(3) . . ? C39 O9 N3 121.6(10) . 1_565 ? C39 O9 C16 132.0(10) . 1_565 ? N3 O9 C16 57.5(2) 1_565 1_565 ? C39 O9 C25 96.3(10) . 1_565 ? N3 O9 C25 44.2(2) 1_565 1_565 ? C16 O9 C25 101.5(3) 1_565 1_565 ? O9 C39 N8 134.3(19) . . ? C39 N8 C40 115.4(18) . . ? C39 N8 C41 126.9(17) . . ? C40 N8 C41 116.0(18) . . ? C42 O10 N1 149.3(12) . . ? C42 O10 C14 112.6(10) . . ? N1 O10 C14 46.8(3) . . ? C42 O10 C2 124.0(11) . . ? N1 O10 C2 54.6(3) . . ? C14 O10 C2 98.2(4) . . ? O10 C42 N9 124.8(10) . . ? C42 N9 C44 121.4(16) . . ? C42 N9 C43 120.4 . . ? C44 N9 C43 118.1(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C1 C9 O1 -12.3(12) . . . . ? C2 C1 C9 O1 164.0(10) . . . . ? C1 C9 N1 C10 178.3(9) . . . . ? O1 C9 N1 C10 -1.4(15) . . . . ? C9 N1 C10 C11 19.3(16) . . . . ? C9 N1 C10 C14 -163.0(9) . . . . ? S7 C15 C23 O2 1.5(12) . . . . ? C16 C15 C23 O2 -175.6(9) . . . . ? C15 C23 N3 C24 -178.1(8) . . . . ? O2 C23 N3 C24 1.7(15) . . . . ? C23 N3 C24 C25 173.1(9) . . . . ? C23 N3 C24 C28 -8.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.235 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.134